CN103267708A - Rapid detection method for noble metal - Google Patents

Rapid detection method for noble metal Download PDF

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Publication number
CN103267708A
CN103267708A CN2013102065631A CN201310206563A CN103267708A CN 103267708 A CN103267708 A CN 103267708A CN 2013102065631 A CN2013102065631 A CN 2013102065631A CN 201310206563 A CN201310206563 A CN 201310206563A CN 103267708 A CN103267708 A CN 103267708A
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sample
unit
detected
samples
density
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李辉
王璇
朱勇
王友建
高成
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Chongqing Academy of Metrology and Quality Inspection
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Chongqing Academy of Metrology and Quality Inspection
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Abstract

The invention discloses a rapid detection method for noble metal. The rapid detection method comprises the following steps of: 1) weighing the mass of a sample to be detected by a precision balance and vacuumizing the sample to be detected; 2) immersing the sample to be detected in distilled water and weighing the mass of the immersed sample by using the precision balance; 3) calculating the actual density of the sample to be detected; 4) detecting the content of the noble metal and impurity elements in the sample to be detected by utilizing an X fluorescence spectrograph and calculating the theoretical density of the sample to be detected; and 5) calculating an error between the actual density and the theoretical density of the sample to be detected, wherein if the error is in a range of 0.5%, testing data of the sample to be detected is accurate. The method disclosed by the invention can detect a plurality of samples to be detected at the same time and can analyze the reliability of detection results of the plurality of samples to be detected from a plurality of angles, so that a final detection conclusion is obtained and the accuracy of detection data is guaranteed; and the data can be rapidly obtained and an effective manner is provided for the development of the mass detection work.

Description

A kind of noble metal method for quick
Technical field
The present invention relates to a kind of quality determining method, relate in particular to a kind of noble metal method for quick.
Background technology
The reality that increases day by day at the precious metal jewelry detection difficulty, technology for detection both domestic and external mechanism is all developing new detection method and detection means targetedly, these technology comprise x ray fluorescence spectrometry, densimetry, chemical method etc., in the hope of can solve a difficult problem of running at a high speed, effectively, accurately in real work.
At present, the noble metal Non-Destructive Testing mainly relies on x ray fluorescence spectrometry and densimetry, and two kinds of methods respectively have relative merits.The advantage of x ray fluorescence spectrometry is simple to operate, and detection speed is very fast, and shortcoming is that the instrument penetration power is poor, only can analyze sample surfaces, can't detect the inside of thicker sample.The own limitation of densimetry and very high to the requirement of sample shape, technology, and can't detect alloy ornament, batch detection efficient is low, and speed is slow; And when adopting the real density of densimetry nondestructive measurement noble metal, because micro-air is assembled on the sample of complicated shape and surface easily, thereby influence measurement accuracy.And chemical method is to diminish detection method, and complicated operation, detects the cost height, does not almost use.Because diversity, the complicacy of sample and reaching its maturity of the technology of playing tricks in the actual detected work uses two kinds of detection methods of fluorescent spectrometry and densimetry not tackle fully respectively.License number: 200820074914 " noble metal nondestructive detection systems " are that the X fluorescence spectrophotometer is connected computing machine, and penetron is connected and connects computing machine on the electronic balance again.These system's characteristics are that the X fluorescence spectrophotometer is except the content of the composition of measuring the sample surfaces layer and each element, data computation goes out to contain the alloy density of this composition thus, this alloy density is compared with the real density that penetron is measured again, judgement sample is entity gold or only skin is enclosed with gold, to solve the sample error-detecting to layer of precious metal.But this noble metal nondestructive detection system can only detect single sample, can not detect simultaneously a plurality of samples and can't realize the defective of fast detecting.
Summary of the invention
At detecting single sample in the prior art, can not detect simultaneously a plurality of samples and can't realize the defective of fast detecting, with and penetron the simple shape sample measurement accurately to complicated shape sample, the particularly inner big defective of sample measurement error that slit and micropore are arranged, be the invention provides a kind of noble metal method for quick of realizing fast, accurately measuring.
In order to solve the problems of the technologies described above, the present invention has adopted following technical scheme:
The noble metal method for quick comprises the steps:
1) adopts precision balance earlier a plurality of samples to be weighed quality in air, adopt vacuum plant to extract the sample ambient air again;
2) then sample is invaded in the distilled water fully by suspender, weigh the quality of these samples in distilled water with precision balance, and with this quality signal input computing machine;
3) calculated the actual density of a plurality of samples simultaneously by following formula by computing machine:
ρ 1 /( mm 1 m 2
In the formula: ρ-tested sample is in temperature tDensity constantly, unit: g/cm 3
mThe aerial quality of-tested sample, unit: g;
m 1 -tested sample is invaded the weighing value in the distilled water, unit: g;
m 2 The weighing value of-suspender in distilled water, unit: g;
ρ 1 -distilled water is in temperature tDensity constantly, unit: g/cm 3
4) utilize the content of noble metal and impurity element in a plurality of samples that the X fluorescence spectrophotometer records and import computing machine, the corresponding content that is undertaken by computing machine converts and calculates the solid density of a plurality of samples by following formula simultaneously:
Figure 2013102065631100002DEST_PATH_IMAGE001
In the formula: ρ x The solid density of-sample, unit: g/cm 3
mThe structure cell quality of-sample, total in the structure cell nPlant atom, unit: g;
VThe unit cell volume of-sample, unit: cm 3
m i In-testing sample the structure cell iThe relative atomic mass summation of element, unit: g/mol;
N 0 -Avogadro's number, 6.022*10 23/ mol;
a x -testing sample grating constant, unit: nm;
Wherein: a x -testing sample grating constant is measured by X-ray diffraction analysis; Utilize X-ray diffraction analysis to measure various common component noble metals a x , form a x Database, and formulate corresponding working curve is in order to extract during fast detecting a x Data;
VThe unit cell volume of-sample, because sample is face-centred cubic structure, so V=a x 3
Figure 765754DEST_PATH_IMAGE002
5) calculate a plurality of testing sample actual densities by computing machine simultaneously by following formula ρWith solid density ρ x Error Δ, in 5 ‰, then the test sample test data is accurate as if both errors;
Δ= ρ x ?- ρ/ ρ x ?。
Compared with prior art, the present invention has following advantage:
1, this noble metal method for quick is compared with the Density Detection method with X fluorescence spectrophotometer method, solved that X fluorescence spectrophotometer method only detects the noble metal top layer and than the limitation of zonule, and densimetry is to the requirement height of sample shape, technology, shortcomings such as batch detection efficient is low, the usable range of expansion densimetry; This method can detect a plurality of testing samples simultaneously, and from the reliability of a plurality of testing sample testing results of multi-angular analysis, thereby obtain final detection conclusion, guaranteed to detect the accuracy of data, and provide data fast, for carrying out of quality detection work provides an effective way.
2, this noble metal method for quick will adopt the system of vacuum densimetry and X fluorescence spectrophotometer, penetron to programme to realize fast, accurately measure.
Description of drawings
Fig. 1 is a kind of process flow diagram of noble metal fast detecting;
Fig. 2 is the structural representation of vacuum plant.
In the accompanying drawing: 1-vacuum pump; 2-lower header; 3-solenoid valve; 4-sales kit (SK); 5-vacuum chamber; 6-illuminating lamp.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is done to describe in further detail.
A kind of noble metal method for quick comprises the steps, as shown in Figure 1:
1) adopts precision balance earlier a plurality of samples to be weighed quality in air, adopt vacuum plant to extract the sample ambient air again.The structure of vacuum plant as shown in Figure 2, vacuum plant comprises vacuum pump 1, lower header 2, solenoid valve 3, sales kit (SK) 4, vacuum chamber 5, illuminating lamp 6 etc., a plurality of samples are weighed quality in air after, put into sales kit (SK) 4 and vacuumize.
2) sample is invaded in the distilled water fully by suspender (by cord sample is hung in distilled water usually) then, weigh the quality of these samples in distilled water with precision balance, and this quality signal is imported computing machine by the transmission of RS232 interface.
3) calculated the actual density of a plurality of samples simultaneously by following formula by computing machine:
ρ 1 /( mm 1 m 2
In the formula: ρ-tested sample is in temperature tDensity constantly, unit: g/cm 3
mThe aerial quality of-tested sample, unit: g;
m 1 -tested sample is invaded the weighing value in the distilled water, unit: g;
m 2 The weighing value of-suspender in distilled water, unit: g;
ρ 1 -distilled water is in temperature tDensity constantly, unit: g/cm 3
4) utilize the content of noble metal and impurity element in a plurality of samples that the X fluorescence spectrophotometer records and import computing machine, the corresponding content that is undertaken by computing machine converts and calculates the solid density of a plurality of samples by following formula simultaneously:
Figure 588217DEST_PATH_IMAGE001
In the formula: ρ x The solid density of-sample, unit: g/cm 3
mThe structure cell quality of-sample, total in the structure cell nPlant atom, unit: g;
VThe unit cell volume of-sample, unit: cm 3
m i In-testing sample the structure cell iThe relative atomic mass summation of element, unit: g/mol;
N 0 -Avogadro's number, 6.022*10 23/ mol;
a x -testing sample grating constant, unit: nm;
Wherein: a x -testing sample grating constant is measured by X-ray diffraction analysis; Utilize X-ray diffraction analysis to measure various common component noble metals a x , form a x Database, and formulate corresponding working curve is in order to extract during fast detecting a x Data;
VThe unit cell volume of-sample, because sample is face-centred cubic structure, so V=a x 3
5) calculate a plurality of testing sample actual densities by computing machine simultaneously by following formula ρWith solid density ρ x Error Δ, in 5 ‰, then the test sample test data is accurate as if both errors;
Δ= ρ x ?- ρ/ ρ x ?;
Computing machine is provided examining report simultaneously according to a plurality of test sample test datas.
This method adopts the hydrostatic weighing method based on Archimedes principle, measures the quality of sample in air in batches with balance, measures its volume by batch weighing sample in liquid (distilled water), calculates the actual density of sample in batches with this.Use X fluorescence spectrophotometer method to draw sample batches noble metal and impurity content, obtain the solid density of sample.The actual density of system-computed batch sample and the error of solid density, in 5 ‰, then the test sample test data is accurate as if both errors.Solved that X fluorescence spectrophotometer method only detects the noble metal top layer and than the limitation of zonule, and densimetry is to the requirement height of sample shape, technology, shortcomings such as batch detection efficient is low, enlarge the usable range of densimetry, the advantage of two kinds of methods of stack, the limitation that the shortcoming of minimizing method own is brought.By experimental results demonstrate, this method can realize accurately, in batches, efficiently, the purpose that fast the noble metal sample detected.
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although with reference to preferred embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not breaking away from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.

Claims (1)

1. a noble metal method for quick is characterized in that, this method comprises the steps:
1) adopts precision balance earlier a plurality of samples to be weighed quality in air, adopt vacuum plant to extract the sample ambient air again;
2) then sample is invaded in the distilled water fully by suspender, weigh the quality of these samples in distilled water with precision balance, and with this quality signal input computing machine;
3) calculated the actual density of a plurality of samples simultaneously by following formula by computing machine:
ρ 1 /( mm 1 m 2
In the formula: ρ-tested sample is in temperature tDensity constantly, unit: g/cm 3
mThe aerial quality of-tested sample, unit: g;
m 1 -tested sample is invaded the weighing value in the distilled water, unit: g;
m 2 The weighing value of-suspender in distilled water, unit: g;
ρ 1 -distilled water is in temperature tDensity constantly, unit: g/cm 3
4) utilize the content of noble metal and impurity element in a plurality of samples that the X fluorescence spectrophotometer records and import computing machine, the corresponding content that is undertaken by computing machine converts and calculates the solid density of a plurality of samples by following formula simultaneously:
Figure 778434DEST_PATH_IMAGE001
In the formula: ρ x The solid density of-sample, unit: g/cm 3
mThe structure cell quality of-sample, total in the structure cell nPlant atom, unit: g;
VThe unit cell volume of-sample, unit: cm 3
m i In-testing sample the structure cell iThe relative atomic mass summation of element, unit: g/mol;
N 0 -Avogadro's number, 6.022*10 23/ mol;
a x -testing sample grating constant, unit: nm;
Figure 2013102065631100001DEST_PATH_IMAGE002
5) calculate a plurality of testing sample actual densities by computing machine simultaneously by following formula ρWith solid density ρ x Error Δ, in 5 ‰, then the test sample test data is accurate as if both errors;
Δ= ρ x ?- ρ/ ρ x ?。
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105403589A (en) * 2015-12-23 2016-03-16 芜湖东旭光电装备技术有限公司 Method for measuring shrinkage of amorphous material
CN105445146A (en) * 2015-12-04 2016-03-30 成都信息工程大学 Novel soft magnetic ring density testing device
CN106959313A (en) * 2017-05-24 2017-07-18 深圳市金质金银珠宝检验研究中心有限公司 A kind of method for quick of objects made from precious metals
WO2019006824A1 (en) * 2017-07-05 2019-01-10 深圳市华唯计量技术开发有限公司 Method and system for rapidly determining material adulteration based on x-ray fluorescence
CN109726457A (en) * 2018-12-17 2019-05-07 深圳市中行建设工程顾问有限公司 A kind of overall process intelligence engineering supervisory information managing and control system
CN111044409A (en) * 2019-12-02 2020-04-21 无锡英特派金属制品有限公司 Method for testing mass fraction of rhodium in platinum-rhodium alloy
CN111051864A (en) * 2017-08-10 2020-04-21 沙特阿拉伯石油公司 Method and system for determining bulk density, porosity and pore size distribution of a subterranean formation

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105445146A (en) * 2015-12-04 2016-03-30 成都信息工程大学 Novel soft magnetic ring density testing device
CN105403589A (en) * 2015-12-23 2016-03-16 芜湖东旭光电装备技术有限公司 Method for measuring shrinkage of amorphous material
CN106959313A (en) * 2017-05-24 2017-07-18 深圳市金质金银珠宝检验研究中心有限公司 A kind of method for quick of objects made from precious metals
WO2019006824A1 (en) * 2017-07-05 2019-01-10 深圳市华唯计量技术开发有限公司 Method and system for rapidly determining material adulteration based on x-ray fluorescence
CN111051864A (en) * 2017-08-10 2020-04-21 沙特阿拉伯石油公司 Method and system for determining bulk density, porosity and pore size distribution of a subterranean formation
US11022716B2 (en) 2017-08-10 2021-06-01 Saudi Arabian Oil Company Methods and systems for determining bulk density, porosity, and pore size distribution of subsurface formations
US11022715B2 (en) 2017-08-10 2021-06-01 Saudi Arabian Oil Company Methods and systems for determining bulk density, porosity, and pore size distribution of subsurface formations
CN111051864B (en) * 2017-08-10 2021-07-16 沙特阿拉伯石油公司 Method and system for determining bulk density, porosity and pore size distribution of a subterranean formation
CN109726457A (en) * 2018-12-17 2019-05-07 深圳市中行建设工程顾问有限公司 A kind of overall process intelligence engineering supervisory information managing and control system
CN111044409A (en) * 2019-12-02 2020-04-21 无锡英特派金属制品有限公司 Method for testing mass fraction of rhodium in platinum-rhodium alloy

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Application publication date: 20130828